ICP-MS测定注射用重组人凝血因子Ⅷ-Fc融合蛋白中7个元素的迁移量  

Determination of migration of 7 elements in recombinant human coagulation factorⅧ-Fc fusion protein for injection by ICP-MS

作　　者：丁豪 DING Hao(Shanghai Food and Drug Packaging Material Control Center,Shanghai 201203,China)

机构地区：[1]上海市食品药品包装材料测试所,上海201203

出　　处：《药物分析杂志》2024年第8期1437-1442,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立电感耦合等离子体质谱(ICP-MS)法测定注射用重组人凝血因子Ⅷ-Fc融合蛋白中钴(Co)、砷(As)、溴(Br)、镉(Cd)、锑(Sb)、钡(Ba)、铅(Pb)的迁移量,并对相容性长期放置的样品进行定量分析。方法:样品加纯化水0.75 mL,倒置复溶4 h后,用纯化水定容至5 mL,采用标准加入法测定待测溶液中7个元素的含量。ICP-MS工作参数:射频功率为1550 W,采样深度为10.0 mm,载气(氩气)流量为0.50 L·min^(-1),雾化器泵速为0.30 r·s^(-1),雾化室温度为2℃,稀释气流量为0.74 L·min^(-1),重复取样次数3次,分析模式为全定量。结果:各元素在各自的检测质量浓度范围内线性关系良好,元素加标回收率在92.0%~101.8%,应用于各加速放置点样品的检测时,除Br元素含量略有增长(增长迁移量分别为43.2、68.7、66.8 ng·mL^(-1))外,其余6个元素含量均远小于规定限度。结论:经方法学验证,本方法结果可靠,可用于注射用重组人凝血因子Ⅷ-Fc融合蛋白样品中7个元素的迁移量测定。Objective:To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of migration Co,As,Br,Cd,Sb,Ba and Pb in recombinant human coagulation factorⅧ-Fc fusion protein for injection,and to quantitatively analyze the compatibility of long-term stored samples.Methods:After adding 0.75 mL of water to the sample for 4 h,the purified water was filled to 5 mL,and the contents of 7 elements in the solution were determined by standard addition method.The working parameters of ICP-MS:radio frequency(RF)power of 1550 W,sampling depth of 10.0 mm,carrier gas flow rate of 0.50 L·min^(-1),atomizer pump speed of 0.30 r·s^(-1),atomization chamber temperature of 2℃,dilution gas flow rate of 0.74 L·min^(-1),repeated sampling times of 3 times,analysis mode of full quantitative.Results:The linear relationship of each element was good in the concentration range of the detected mass,and the recoveries of the element added were 92.0%-101.8%.When applied to the determination of the samples at each accelerated placement point,the increased migration amounts were 43.2,68.7 and 66.8 ng·mL^(-1),respectively,except the element content of Br increased slightly.The contents of the remaining 6 elements were far below the prescribed limit.Conclusion:The method is reliable and can be used for the determination of migration of 7 elements in recombinant human coagulation factorⅧ-Fc fusion protein for injection.

关 键 词：电感耦合等离子体质谱 注射用重组人凝血因子Ⅷ-Fc融合蛋白 元素杂质 相容性 迁移量 

分 类 号：R917[医药卫生—药物分析学]